EP2751331B2 - Kraft-kochverfahren mit einer polysulfidkochlauge - Google Patents

Kraft-kochverfahren mit einer polysulfidkochlauge Download PDF

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Publication number
EP2751331B2
EP2751331B2 EP11871390.8A EP11871390A EP2751331B2 EP 2751331 B2 EP2751331 B2 EP 2751331B2 EP 11871390 A EP11871390 A EP 11871390A EP 2751331 B2 EP2751331 B2 EP 2751331B2
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EP
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Prior art keywords
cooking
liquor
polysulfide
alkali
impregnation stage
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English (en)
French (fr)
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EP2751331B1 (de
EP2751331A1 (de
EP2751331A4 (de
Inventor
Mikael Lindström
Fredrik Wilgotson
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Valmet Technologies Oy
Valmet AB
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Valmet Oy
Valmet AB
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00—Pretreatment of the finely-divided materials before digesting
    • D21C1/06—Pretreatment of the finely-divided materials before digesting with alkaline reacting compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes

Definitions

  • the present invention relates to a method for the preparation of kraft pulp with increased pulping yield from lignin-containing cellulosic material using polysulfide cooking liquor.
  • Cooking methods was therefore developed in order to reduce the detrimental high alkali peak concentrations at start of the cook, and thus was split charges of alkali during the cook implemented in cooking methods such as MCC, EMCC, ITC and Lo-Solids cooking.
  • alkali consumption during the cooking process i.e. including impregnation
  • a large part of the alkali consumption is due to the initial neutralization of the wood acidity, and as much as 50-75% of the total alkali consumption is occurring during the neutralization process.
  • a lot of alkali is needed to be charged to the initial neutralization. This establish a cumbersome problem as high alkali concentrations had been found to be detrimental for pulp viscosity when charged to top of digesters in conventional cooking.
  • alkali treatment liquors preferably black liquor having a residual alkali content, but having low alkali concentration, which resulted in presence of relatively large amount of total alkali per kg of wood material but still at low alkali concentration.
  • Metso disclosed a pretreatment stage using polysulfide cooking liquor ahead of black liquor treatment.
  • the polysulfide treatment liquor drained after the pretreatment stage and before starting the black liquor treatment.
  • the polysulfide treatment stage was also preferably kept short with treatment time in the range 2-10 minutes.
  • US 3664919 A discloses a method for impregnating lignocellulosic material, previously saturated with water, in a first stage with an alkaline polysulphide cooking liquor, removing excess liquor, and then cooking the impregnated material in a second stage by rapidly heating with steam.
  • C A2763651 A1 discloses a continuous digestion method using a digester equipped inside with a top zone, an upper digestion zone, a lower digestion zone, and a digestion/cleaning zone which have been arranged in this order from the top toward the bottom, each zone having a strainer disposed at the bottom, and a black liquor extracted through at least one of the strainers being discharged from the digestion system.
  • US 3567572 A discloses a process for the production of cellulosic pulp from lignocellulosic materials which comprises substantially completely impregnating said materials in subdivided form with a polysulphide liquor containing no added sodium hydroxide at a temperature below that at which substantial decomposition of the polysulphide occurs, removing excess polysulphide liquor from the impregnated materials, stabilizing the impregnated materials against alkaline degradation by increasing the temperature of said materials and subsequently delignifying said stabilized materials by cooking said material in a cooking liquor containing sodium hydroxide.
  • US 2009/126883 A1 discloses a method for Kraft pulping, wherein the total required alkali charge is added to the beginning of a cook, and after all polysulfide has essentially reacted with lignocellulosic material at temperature below that at which no significant carbohydrate degradation occurs, a first quantity of the cooking liquor high in effective alkali concentration is removed from a first point in the pulping process and replaced with a cooking liquor low in effective alkali concentration removed from another process point.
  • WO 99/14423 A1 discloses a process for producing pulp from cellulosic fiber, wherein the cellulosic fiber material is impregnated with polysulfide before cooking followed by extraction of spent cooking liquor. A portion of the spent cooking liquor is gasified to hydrogen sulphide and treated to form an acidic gas comprising hydrogen sulphide and carbon dioxide.
  • WO 03/057979 A1 discloses a method for the manufacture of cooked cellulose pulp in which the starting material undergoes a successive increase in temperature towards cooking temperature while the chips are first treated in a pre-treatment zone in which the main part, greater than 50%, of fresh white liquor necessary for the cooking stage is added, after which this alkali-rich treatment fluid is withdrawn and replaced to a major extent by black liquor.
  • the present invention is provided by the appended claim 1.
  • Beneficial embodiments are provided in the dependent claims. Accordingly, the invention is based upon the surprising finding that concentration of polysulfide should be kept high in a low temperature pretreatment stage at relatively long retention time before cooking, using liquor to wood ratios well below that as commonly used.
  • the stabilization effect of carbohydrates the major objective for polysulfide addition, has shown to be improved dramatically if using a liquor to wood ratio of about 2,9 instead of the conventional liquor to wood ratio of about 3,5, and all other conditions equal. This non proportional effect of low liquor to wood ratio has not been disclosed or realized before despite the numerous proposals for improving cooking yield using polysulfide cooking liquor.
  • One object of the present invention is to provide an improved method for the preparation of kraft pulp with increased pulping yield from lignin-containing cellulosic material using polysulfide cooking liquor, wherein the lignin-containing cellulosic material is heated to a temperature in the range 50-100 °C followed by adding polysulfide cooking liquor to a first impregnation stage which in turn is followed by cooking stages resulting in a kraft pulp with a kappa number below 40, and wherein the impregnation stage is conducted at high alkali concentration, low temperature and high polysulfide concentration using polysulfide cooking liquor at a liquor-to-wood ratio in the range 2.0 to 3.2 , and that the temperature is between 80-120°C during a retention time resulting in a H-factor in the range 2-20 and preferably 2-10 of the impregnation stage.
  • This low H-factor is indicative for that no cooking or delignification effect is obtained in the first impregnation stage, and hence is no reduction in pulp viscosity seen as could be the case if high alkali concentrations are at hand in cooking stages at higher temperatures.
  • the effective alkali concentration during the impregnation stage is above 60 g/l when adding the polysulfide cooking liquor.
  • the polysulfide concentration during the impregnation stage is above 3 g/l, or above 0,09 mol/l, when adding the polysulfide cooking liquor.
  • more than 90% of the total charge of cooking liquor needed for completion of the cooking stages to the intended kappa number below 40 is charged to the first impregnation stage, and that at least 175 kg of alkali (EA as NaOH) per ton of chips is charged for softwood and at least 160 kg of alkali per ton of chips for hardwood.
  • EA alkali
  • the alkali concentration reduced by at least 8 g/l by adding additional cooking liquids having less alkali concentration than the alkali concentration prevailing at end of the first impregnation stage when increasing the temperature to cooking temperature, said cooking liquids in at least part thereof includes black liquor.
  • the inventive method has also preferably the white liquor added to the first impregnation stage an alkali concentration above 100 g/l and a polysulfide concentration above 4 g/l.
  • the lignin-containing cellulosic materials to be used in the present process are suitably softwood, hardwood, or annual plants.
  • FIG 1 a 2-vessel kraft cooking system, having a first hydraulic impregnation vessel B and a second steam/liquid phase digester C, wherein the inventive method could be implemented.
  • this type of system is first the lignin containing cellulosic material Ch fed to a bin A wherein the cellulosic material is heated to a temperature in the range 50-100 °C by using addition of steam St.
  • the lignin containing cellulosic material could preferably be wood chips.
  • the treatment liquor here is preferably only polysulfide cooking liquor, WL, and preferably is the entire charge of cooking liquor needed for the cooking process charged here.
  • the chips suspended in the treatment liquor are fed to the sluice feeder and displaced liquid is fed out from the bottom outlet of the sluice feeder and returned to the chute in a low pressure circulation.
  • the chips in the sluice feeder is pressurized by the return flow from the vessel B and fed out to the top separator TS in top of the vessel B.
  • the first impregnation stage is implemented in the vessel B and preferably only with the polysulfide cooking liquor and as small amount as possible of additional liquids such as wood moisture, steam condensates, and especially no black liquor nor additional water or filtrates.
  • the resulting liquor-to-wood ratio established should be in the range 2.0 to 3.2 and the temperature should be in the range 80-120°C.
  • the impregnated chips will be fed to the steam/liquid phase digester C together with the residual treatment liquor.
  • a conventional transfer system with dilution in bottom of the vessel B using withdrawn treatment liquor from the top separator TS in the top of vessel C.
  • the chip suspension heated to full cooking temperature, in the range 140-170°C depending upon type of cellulosic material, and additional liquid is added in order to reduce the alkali concentration at this point.
  • a digester C with 2 concurrent cooking zones, one cooking zone above the first screen section and a second cooking zone above the final screen section in bottom of digester.
  • a final counter current wash zone implemented in bottom of digester by addition of wash water/Wash.
  • the final pulp with a kappa number below 40 is fed out from bottom in flow Pu.
  • FIG 2 is disclosed the alkali concentration profile that could be established in a system like that disclosed in figure 1 , with alkali consumption of about 110 kg/BDT in the impregnation vessel, 45 kg/BDT in the first cooking zone in vessel C and 15 kg/BDT in last cooking zone in vessel C.
  • alkali consumption of about 110 kg/BDT in the impregnation vessel, 45 kg/BDT in the first cooking zone in vessel C and 15 kg/BDT in last cooking zone in vessel C.
  • In the top of the first impregnation vessel B is an alkali concentration of about 67 g/l established and this alkali level drops down to about 32 g/l in the bottom of vessel B, where a dilution is made by return flows added to bottom.
  • the cooking in top of digester starts at an alkali concentration of about 22 g/l.
  • figure 3 is disclosed the improved carbohydrate yield as a function of the polysulfide concentration, when about 1% lignin is still present in the pulp.
  • the dramatic increase in yield when increasing the polysulfide concentration above 0,15 mol/L There is basically a linearly increasing yield when the concentration increases between 0 to 0,15 mol/l. In this initial range is the yield increased from about 45% up to about 46.2%. However, when the concentration reach 0,2 mol/L is the yield increased to about 48,3%.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)

Claims (3)

  1. Verfahren zur Gewinnung eines Kraftzellstoffs mit erhöhter Zellstoffausbeute aus Lignin enthaltenden Cellulosematerial unter Verwendung einer Polysulfid-Kochlauge, wobei das Lignin enthaltenden Cellulosematerial auf eine Temperatur in dem Bereich von 50-100°C erhitzt wird, gefolgt vom Hinzufügen von Polysulfid-Kochlauge zu einer ersten Imprägnationsstufe, die wiederrum gefolgt ist von Kochstufen, was in einem Kraftzellstoff resultiert, der eine Kappa-Zahl von unter 40 aufweist, dadurch gekennzeichnet, dass
    die Imprägnationsstufe mit einer hohen effektiven Alkalikonzentration von über 60 g/l durchgeführt wird, wenn die Polysulfid-Kochlauge hinzugefügt wird, geringer Temperatur und hoher Polysulfid-Konzentration über 3g/l oder 0,09 mol/l, wenn die Polysulfid-Kochlauge hinzugefügt wird, unter Verwendung von Polysulfid-Kochlauge bei einem Laugezu-Holz-Verhältnis in dem Bereich 2,0 bis 3,2, und dass die Temperatur während einer Verweilzeit zwischen 80-120°C liegt, was in einem H-Faktor in dem Bereich von 2-20, bevorzugt 2-10 der Imprägnationsstufe resultiert,
    wobei mehr als 90% der Gesamtladung der Kochlauge, die zum Abschluss der Kochstufen zu der angestrebten Kappa-Zahl von unter 40 benötigt wird, in der ersten Imprägnationsstufe hinzugegeben wird, und dass wenigstens 175 Kg von effektivem Alkali (EA als NaOH) für Weichholz und 160 Kg von effektivem Alkali für Hartholz pro Tonne Chips hinzugegeben werden, und
    wobei die Alkalikonzentration um wenigstens 8 g/l reduziert wird durch Hinzufügen zusätzlicher Kochlaugen mit geringerer Alkalikonzentration als die Alkalikonzentration, die am Ende der ersten Imprägnationsstufe vorherrscht, wenn die Temperatur auf Kochtemperatur erhöht wird, wobei die Kochlaugen wenigstens in Teilen davon Schwarzlauge enthalten.
  2. Verfahren gemäß Anspruch 1, wobei zu der ersten Imprägnationsstufe keine Schwarzlauge hinzugefügt wird.
  3. Verfahren gemäß Anspruch 2, wobei die Polysulfid-Kochlauge, die zu der ersten Imprägnationsstufe hinzugefügt wird, eine Alkalikonzentration von über 100 g/l und eine Polysulfid-Konzentration von über 4 g/l aufweist.
EP11871390.8A 2011-08-30 2011-08-30 Kraft-kochverfahren mit einer polysulfidkochlauge Active EP2751331B2 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/SE2011/051038 WO2013032377A1 (en) 2011-08-30 2011-08-30 Kraft cooking method using polysulfide cooking liquor

Publications (4)

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EP2751331A1 EP2751331A1 (de) 2014-07-09
EP2751331A4 EP2751331A4 (de) 2015-05-20
EP2751331B1 EP2751331B1 (de) 2017-06-14
EP2751331B2 true EP2751331B2 (de) 2020-04-22

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US (1) US20140299283A1 (de)
EP (1) EP2751331B2 (de)
JP (1) JP5989777B2 (de)
CN (1) CN103827388B (de)
WO (1) WO2013032377A1 (de)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016032374A1 (en) * 2014-08-26 2016-03-03 Valmet Ab Cost efficient kraft cooking method using polysulfide cooking liquor
FI129362B (fi) * 2017-05-16 2021-12-31 Andritz Oy Menetelmä kemiallisen massan tuottamiseksi
SE543159C2 (en) * 2019-05-22 2020-10-13 Valmet Oy A method for extracting hydrolyzate, a batch cooking system and a hydrolyzate extracting arrangement

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7828930B2 (en) † 2007-11-20 2010-11-09 International Paper Company Use of polysulfide in modified cooking

Family Cites Families (9)

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Publication number Priority date Publication date Assignee Title
US3567572A (en) 1967-09-06 1971-03-02 Pulp Paper Res Inst Polysulfide liquor impregnation of lignocellulose materials in a multistage pulping process
US3664919A (en) * 1969-12-09 1972-05-23 Pulp Paper Res Inst Vapor phase polysulphide liquid pulping of lignocellulosic materials
NO131612C (de) * 1969-12-09 1975-06-25 Pulp Paper Res Inst
JP3064607B2 (ja) * 1991-11-25 2000-07-12 王子製紙株式会社 修正クラフト法パルプの製造方法
US5660686A (en) * 1994-09-02 1997-08-26 Ahlstrom Machinery Inc. Cooking with spent liquor pretreatment of cellulose material
AU9195598A (en) 1997-09-18 1999-04-05 Kvaerner Pulping Ab Polysulfide pulping process
JP4298059B2 (ja) * 1999-05-28 2009-07-15 日本製紙株式会社 リグノセルロース材料の蒸解法
SE518538C2 (sv) 2001-12-14 2002-10-22 Kvaerner Pulping Tech Förbehandling av flis med färsk vitlut före behandling med svartlut
CN102449231B (zh) * 2009-05-26 2014-05-14 日本制纸株式会社 木化纤维素材料的蒸煮法

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7828930B2 (en) † 2007-11-20 2010-11-09 International Paper Company Use of polysulfide in modified cooking

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
WATANABE, K. ET AL.: "Development of a New Cooking System using Highly Concentrated Polysulfide (I)", TAPPI JAPAN JOURNAL, December 2008 (2008-12-01), pages 1557 - 1569, XP055472088 †

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US20140299283A1 (en) 2014-10-09
CN103827388B (zh) 2016-09-21
EP2751331B1 (de) 2017-06-14
EP2751331A1 (de) 2014-07-09
JP2014525519A (ja) 2014-09-29
JP5989777B2 (ja) 2016-09-07
EP2751331A4 (de) 2015-05-20
WO2013032377A1 (en) 2013-03-07
CN103827388A (zh) 2014-05-28

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